CN109534378A - A kind of preparation method of anti-hard aggregation nano alumina particles - Google Patents
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Abstract
The present invention relates to a kind of preparation methods of anti-hard aggregation nano alumina particles, comprising: prepares AlCl respectively3Solution and NH4HCO3Solution；Adjust NH4HCO3Solution ph, and dispersing agent is added, obtain mixed solution；By AlCl3Solution is added dropwise in mixed solution, and ageing obtains presoma, washing, drying, grinding, calcine to get.Preparation process of the present invention is easy to operate, and reaction condition is mild, efficiently solves the problems, such as nanoparticle agglomerates, is conducive to industrialized application.
Description
Technical field
The invention belongs to the preparation field of nano aluminium oxide, in particular to a kind of system of anti-hard aggregation nano alumina particles
Preparation Method.
Background technique
Since nano material has different from conventional special performance --- bulk effect, quantum size effect, surface circle
It face effect and macroscopical tunnel-effect etc. and its various important answers electronics, optics, chemical industry, ceramics, biology and medicine etc. are all
With and cause the great attention of people.In recent years, the extensive use of nano aluminium oxide brings a brand-new direction of scientific rersearch, receives
The progress of rice science and technology produces far-reaching influence to aluminium oxide industry.As the nano aluminium oxide of special type function material, tool
There are many excellent characteristics such as high rigidity, high intensity, corrosion-resistant, wear-resistant, high temperature resistant, high-insulativity, high antioxidant, therefore
Widespread adoption is in high technology ceramics, bioceramic, chemical catalyst, refractory material, integrated circuit and aerospace etc..Mesh
The preceding method for preparing nano-powder has: vapour deposition process, plasma method, sol-gel method, hydrothermal synthesis method and chemical coprecipitation
Shallow lake method etc..But since nano-powder has very high specific surface area, belongs to Unstable Systems, be easy to happen serious reunion
Phenomenon, forms that partial size is larger and offspring in irregular shape.The reunion of particle can be divided into soft-agglomerated and hard aggregation, soft-agglomerated
Mainly caused by intergranular electrostatic force and Van der Waals force, since active force is weaker, by some chemical actions or it can apply
The mode of mechanical energy is added to eliminate；The reason of hard aggregation formation other than electrostatic force and Van der Waals force, there is also chemical bond,
Therefore hard aggregation is not easy to be destroyed, and needs that some special methods is taken to be controlled.Therefore, nano-scale oxygen how is prepared
Changing alumina particles and avoiding agglomeration is one of most concerned problem of researcher.
The precipitation method be precipitating reagent appropriate is added in material solution so that in feed liquid cation formed sediment, then
Desired product is obtained by the techniques such as being filtered, washed, drying, be calcined.This method particularly may be divided into direct precipitation method, uniformly sink
Shallow lake method etc..Due to including the links such as precipitation reaction, the washing of grain growth to wet powder, drying, calcination in technical process, all may be used
To lead to the formation of particle grown up and reunited, to obtain the particle system of even particle size distribution, the process control needs: (A)
Nucleation process and growth course separation promote nucleation, control growth；(B) inhibit the reunion of particle.
Liquid phase method be chiefly used in synthesis of solid powder, but participate in reaction raw material be in the form of liquid phase existing for system
Preparation Method.Liquid phase method can be generally divided into hydrothermal synthesis method, sol-gel processing, ion-exchange, the precipitation method, supercritical methanol technology,
High-gravity technology method etc..Wherein the precipitation method are exactly that precipitating reagent appropriate is added in metal salt solution, obtain presoma precipitating, then
Pyrolysis calcining sediment obtains nano alumina powder jointed.The precipitation method are because cost of material is low, equipment and simple process, are easy to industry
Change, in production high-purity superfine alumina powder end Shi Youqi advantage.But the existence form of the reactant of the precipitation method be liquid, can because
It is severe that hydroxyl effect makes product obtained reunite, and obtains the nano-powder product that particle is uneven, particle size is inconsistent.And
The presoma of aluminium oxide prepared by the precipitation method is also easy to happen hard aggregation phenomenon in drying, calcination process.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of preparation method of anti-hard aggregation nano alumina particles, gram
It takes current liquid phase method and prepares during nano aluminium oxide hydroxyl effect during precipitation reaction, alumina precursor dry and forge
Agglomeration traits caused by during burning, the preparation method is simple, short preparation period, it is low in cost, obtain anti-hard aggregation, nanometer ruler
Very little lesser alumina particle.
A kind of preparation method of nano alumina particles of the invention, comprising:
(1) anhydrous AlCl3And NH4HCO3For raw material, AlCl is prepared respectively3Solution and NH4HCO3Solution；
(2) NH is adjusted4HCO3Solution ph, and dispersing agent is added, obtain mixed solution；
(3) by AlCl3Solution is added dropwise in step (2) mixed solution, and ageing obtains presoma, wash, drying, grind,
Calcining is to get nano aluminium oxide γ-Al2O3Particle.
The preferred embodiment of above-mentioned preparation method is as follows:
AlCl in the step (1)3The concentration of solution is 1-2mol/L, in order to guarantee Al during reacting progress3+Energy
Enough reactions are abundant, so that precipitating reagent NH4HCO3Solution is in hypersaturated state, NH always4HCO3The concentration of solution is 6-7mol/
L, AlCl3Solution and NH4HCO3The volume ratio of solution is 1:1.
NH is adjusted in the step (2)4HCO3PH value of solution is to adjust pH=7-9.5 using ammonium hydroxide.
Dispersing agent is surfactant in the step (2).
Dispersing agent is one or more of different molecular weight PEG in the step (2), and the additional amount of dispersing agent is
AlCl3+
NH4HCO3+H2The 0.1%-1% of the gross mass of O.
It is preferred that the dispersing agent is PEG300, PEG2000.
The mass ratio of further preferred dispersing agent PEG300, PEG2000 are 1:1.
It is added dropwise in the step (3) specifically: by AlCl3Solution is placed in constant pressure titration funnel, with 1-4 drop/s speed
It is added drop-wise in step (2) solution；Digestion time is 10-30min.
It is preferred that: with the dropwise addition of 2 drops/s speed；Digestion time is 30min, guarantees that reaction is thorough.
Washing is that deionized water is washed in the step (3), and then dehydrated alcohol is washed；Drying temperature is 80-90
℃；Calcining is to be warming up to 600-650 DEG C in Muffle furnace with the heating rate of 5-10 DEG C/min, calcines 0.5-3h.
It is preferred that: drying temperature is 90 DEG C；Calcining is to be warming up to 650 DEG C in Muffle furnace with the heating rate of 10 DEG C/min, is forged
Burn 2h.
The present invention provides a kind of nano alumina particles of the method preparation.
It is described that presoma is first washed with deionized, the foreign ion in presoma is removed, then washed with dehydrated alcohol, kept away
Exempt to make to be tightly combined between particle due to the hydrogen bond action of water, leads to the formation of last chemical bond.Meanwhile organic agent functional groups (-
OC2H5)
The non-bridge formation hydroxyl of micelle surface portion can be replaced, and certain steric hindrance can be played the role of, can reduce in this way
Or eliminate the generation of hard aggregation.
The meso-position radius of the nano aluminium oxide is 3-40nm.
The present invention also provides a kind of applications of the nano alumina particles of the method preparation.Nano alumina particles are used
In the separating layer for preparing nanofiltration membrane.It is well known that the partial size of inorganic particle has extremely important shadow for ceramic membrane pore structure
It rings, the particle diameter distribution of powder determines the pore size of ceramic membrane, and smaller diameter of particle is to generate smaller ceramics in inorganic raw material
The premise of membrane pore structure.Preparing ceramic membrane with nano aluminium oxide enables to sintering temperature to reduce, usual alumina sintering temperature
At 1700 DEG C or so, and nano aluminium oxide can be sintered at 1200 DEG C or so, and consistency enables to material up to 99%
Mechanical property is greatly enhanced.For nanofiltration film preparation, inorganic particle partial size used by ceramic membrane separation layer
It is necessary for nanoscale subparticle, and the particle size of powder must be concentrated and have good dispersibility.This method is made
Standby nano aluminium oxide is suitable as the separating layer aggregate of nanofiltration membrane.
Beneficial effect
Preparation process of the present invention is easy to operate, and reaction condition is mild, by prepared nano alumina particles progress
SEM, TEM, XRD characterization analysis, by characterization result it is found that this method efficiently solves the problems, such as nanoparticle agglomerates, are conducive to work
The application of industry.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is alumina precursor TG-DSC curve；
Fig. 3 is the γ-Al obtained using PEG2000 as dispersing agent2O3SEM photograph；
Fig. 4 is the γ-Al obtained using PEG2000 as dispersing agent2O3XRD spectra；
Fig. 5 is the γ-Al for not adding dispersing agent acquisition2O3SEM photograph；
Fig. 6 is the γ-Al obtained with PEG2000 and PEG300 collectively as dispersing agent2O3TEM photo；Wherein illustration is
Partial enlarged view；
Fig. 7 is the γ-Al obtained with PEG2000 and PEG300 collectively as dispersing agent2O3Grading curve；Wherein
Illustration is partial size statistics；
Fig. 8 is the γ-Al obtained with PEG2000 and PEG300 collectively as dispersing agent2O3XRD spectra.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
The NH that quality is 25.7204g is weighed4HCO3Powder granule is dissolved in the deionized water of 48.2mL and is made into concentration
For 6.75mol/L supersaturation NH4HCO3Solution；The anhydrous AlCl that quality is 9.6398g is weighed3Powder is slowly added to be equipped with
In the beaker of the deionized water of 48.2mL, the side Bian Tianjia stirring and dissolving prevents exothermic dissolution from solution temperature being caused sharply to increase, matches
The AlCl for being 1.5mol/L at concentration3Solution；
NH is adjusted with ammonium hydroxide4HCO30.2636gPEG2000 is added as dispersing agent, by AlCl to 8 in the pH value of solution3
Solution is placed in constant pressure separatory funnel, is added to NH with 2 drops/s rate4HCO3In solution, the magnetic agitation when being added dropwise is added dropwise
After, it is aged 30min.Sediment obtained is washed with deionized 1-2 times, is separated by solid-liquid separation with Buchner funnel, then
It is washed 1-2 times with dehydrated alcohol, is equally separated by solid-liquid separation.Resulting sediment is put into drying in 90 DEG C of constant temperature ovens, is ground
Alumina precursor powder aluminium carbonate ammonium is obtained after mill.For determine nano aluminium oxide precursor powder calcination temperature, first to it
Thermogravimetric analysis is carried out, gained TG-DSC curve graph is as shown in Figure 2.According to TG-DSC curve, it is found that with the liter of temperature
Height, by-product gradually decompose vaporization, and when temperature reaches 600 DEG C, the mass loss of powder tends towards stability, and powder quality no longer subtracts
It is few, therefore calcination temperature is selected to guarantee that presoma decomposition reaction can be carried out sufficiently for 650 DEG C.Then it puts it into Muffle furnace
650 DEG C are warming up to the heating rate of 10 DEG C/min, calcines 2h to get nanometer γ-Al2O3Powder carries out prepared particle
SEM, XRD test analysis, Fig. 3 are the γ-Al obtained using PEG2000 as dispersing agent2O3SEM photograph, discovery particle size with
Shape homogeneity is preferable, and dispersibility preferably, partially there is agglomeration, particle size range 30-40nm.Fig. 4 be using PEG2000 as
γ-the Al that dispersing agent obtains2O3XRD spectra, by with standard diagram comparison known to product be monocrystalline type γ-Al2O3, have no
Other miscellaneous peaks, and peak type is significantly broadened, this is the performance of particle refinement.And by XRD characterization map it is found that most strong diffraction maximum
Intensity is 1094.3, interplanar distance d=2.4400, and halfwidth FWHM is 0.272 °, i.e. 0.00475rad, most strong diffraction maximum pair
The 2 θ value of the angle of diffraction answered be 36.805 °, θ be 18.4025 °, calculate average primary particle diameter having a size of 30.42nm.This and SEM table
It is essentially identical to levy result.
Embodiment 2
The NH that quality is 23.1542g is weighed4HCO3Powder granule is dissolved in the deionized water of 43.4mL and is made into concentration
For 6.75mol/L supersaturation NH4HCO3Solution；The anhydrous AlCl that quality is 8.6804g is weighed3Powder is slowly added to be equipped with
In the beaker of the deionized water of 43.4mL, the side Bian Tianjia stirring and dissolving prevents exothermic dissolution from solution temperature being caused sharply to increase, matches
The AlCl for being 1.5mol/L at concentration3Solution；
NH is adjusted with ammonium hydroxide4HCO3The pH value of solution is added without dispersing agent to 8, by AlCl3Solution is placed in constant pressure liquid separation leakage
In bucket, NH is added to 2 drops/s rate4HCO3In solution, the magnetic agitation when being added dropwise after being added dropwise, is aged 30min.It will
Sediment obtained is washed with deionized 1-2 times, is separated by solid-liquid separation with Buchner funnel, then is washed 1-2 times with dehydrated alcohol,
Equally it is separated by solid-liquid separation.Resulting sediment is put into drying in 90 DEG C of constant temperature ovens, alumina precursor powder is obtained after grinding
Last aluminium carbonate ammonium.Then it puts it into Muffle furnace and is warming up to 650 DEG C with the heating rate of 10 DEG C/min, calcine 2h to get receiving
Rice γ-Al2O3Powder.Gained alumina powder SEM test is subjected to, as shown in Figure 5.It was found that agglomeration is more serious, shape
At offspring, meso-position radius is in 1.73um.
Embodiment 3
The NH that quality is 20.0228g is weighed4HCO3Powder granule is dissolved in the deionized water of 37.5mL and is made into concentration
For 6.75mol/L supersaturation NH4HCO3Solution；The anhydrous AlCl that quality is 7.467g is weighed3Powder is slowly added to be equipped with
In the beaker of the deionized water of 37.5mL, the side Bian Tianjia stirring and dissolving prevents exothermic dissolution from solution temperature being caused sharply to increase, matches
The AlCl for being 1.5mol/L at concentration3Solution；
NH is adjusted with ammonium hydroxide4HCO30.1025gPEG2000 and 0.1025gPEG300 conduct is added to 8 in the pH value of solution
Dispersing agent, by AlCl3Solution is placed in constant pressure separatory funnel, is added to NH with 2 drops/s rate4HCO3In solution, when being added dropwise
Magnetic agitation after being added dropwise, is aged 30min.Sediment obtained is washed with deionized 1-2 times, with Buchner funnel into
Row is separated by solid-liquid separation, then is washed 1-2 times with dehydrated alcohol, is equally separated by solid-liquid separation.Resulting sediment is put into 90 DEG C of constant temperature
It is dry in baking oven, alumina precursor powder is obtained after grinding.Then it puts it into Muffle furnace with the heating rate of 10 DEG C/min
650 DEG C are warming up to, calcines 2h to get nanometer γ-Al2O3Powder.
TEM, XRD test analysis are carried out to prepared particle, Fig. 6 is with PEG2000 and PEG300 collectively as dispersing agent
γ-the Al of acquisition2O3TEM photo, discovery particle size it is very good with shape homogeneity, monodispersity is very good, substantially without group
Poly- phenomenon, particle size range 1-8nm carry out partial size statistics, statistical result such as Fig. 7 institute with Nano Measurer software to Fig. 6
Show, particle diameter distribution is between 1-8nm, average grain diameter 3.76nm.Fig. 8 is with PEG2000 and PEG300 collectively as dispersing agent
γ-the Al of acquisition2O3XRD spectra, the intensity of most strong diffraction maximum is 925.33, interplanar distance d=3.0274, halfwidth
FWHM is 0.100 °, i.e. 0.001745rad, and the corresponding 2 θ value of the angle of diffraction of most strong diffraction maximum is 29.480 °, and θ is 14.740 °, meter
Calculate average primary particle diameter having a size of 8.123nm.This is essentially identical with TEM characterization result.
Claims (10)
1. a kind of preparation method of nano alumina particles, comprising:
(1) AlCl is prepared respectively3Solution and NH4HCO3Solution；
(2) NH is adjusted4HCO3PH value of solution, and dispersing agent is added, obtain mixed solution；
(3) by AlCl3Solution is added dropwise in step (2) mixed solution, ageing, obtains presoma, and washing, grinding, is calcined at drying,
Up to nano aluminium oxide γ-Al2O3Particle.
2. preparation method according to claim 1, which is characterized in that AlCl in the step (1)3The concentration of solution is 1.0-
2.0mol/L；NH4HCO3The concentration of solution is 6.0-7.0mol/L, AlCl3Solution and NH4HCO3The volume ratio of solution is 1:1.
3. preparation method according to claim 1, which is characterized in that adjust NH in the step (2)4HCO3PH value of solution is to adopt
PH=7-9.5 is adjusted with ammonium hydroxide.
4. preparation method according to claim 1, which is characterized in that dispersing agent is different molecular weight PEG in the step (2)
One or more of, the additional amount of dispersing agent is AlCl3+NH4HCO3+H2The 0.1%-1% of the gross mass of O.
5. preparation method according to claim 4, which is characterized in that the dispersing agent is PEG300, PEG2000.
6. preparation method according to claim 1, which is characterized in that be added dropwise in the step (3) specifically: by AlCl3Solution
It is placed in constant pressure titration funnel, is added drop-wise in step (2) solution with 1-4 drop/s speed；Digestion time is 10-30min.
7. preparation method according to claim 1, which is characterized in that washing is that deionized water is washed in the step (3), so
Dehydrated alcohol is washed afterwards；Drying temperature is 80-90 DEG C；Calcining is to be heated up in Muffle furnace with the heating rate of 5-10 DEG C/min
To 600-650 DEG C, 0.5-3h is calcined.
8. a kind of nano alumina particles of claim 1 the method preparation.
9. nano alumina particles according to claim 8, which is characterized in that the meso-position radius of the nano aluminium oxide is 3-
40nm。
10. a kind of application of the nano alumina particles of claim 8.
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Cited By (3)
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| CN114604881A (en) * | 2022-03-24 | 2022-06-10 | 昆明理工大学 | Preparation method of hydroxyl nano-alumina with controllable hydroxyl content |
| CN115818687A (en) * | 2022-11-11 | 2023-03-21 | 济南大学 | Superfine alpha-Al 2 O 3 Preparation method of nano powder |
| CN118045581A (en) * | 2024-04-02 | 2024-05-17 | 山东公泉化工股份有限公司 | Catalyst carrier with porous structure and preparation method thereof |
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